ASTM D3329-03(2017)
(Test Method)Standard Test Method for Purity of Methyl Isobutyl Ketone by Gas Chromatography
Standard Test Method for Purity of Methyl Isobutyl Ketone by Gas Chromatography
SIGNIFICANCE AND USE
4.1 This test method provides a measurement of commonly found impurities in commercially available methyl isobutyl ketone. The measurement of these impurities and the results thereof can individually or when totaled and subtracted from 100 (assay) be used for specification acceptance.
SCOPE
1.1 This test method covers the determination of the purity of methyl isobutyl ketone (MIBK) by gas chromatography and in addition provides a means for measuring certain impurities such as methyl isobutyl carbinol which are of interest. Impurities such as water and acidity are measured by other appropriate ASTM procedures and the results are used to normalize the chromatographic value.
1.2 The following applies to all specified limits in this standard; for purposes of determining conformance with this standard, an observed value or a calculated value shall be rounded off “to the nearest unit” in the last right-hand digit used in expressing the specification limit, in accordance with the round-off method of Practice E29.
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.5 For specific hazard information and guidance, see the supplier’s Safety Data Sheet for the materials listed in this test method.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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Designation: D3329 − 03 (Reapproved 2017)
Standard Test Method for
1,2
Purity of Methyl Isobutyl Ketone by Gas Chromatography
This standard is issued under the fixed designation D3329; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope 2. Referenced Documents
1.1 This test method covers the determination of the purity 2.1 ASTM Standards:
of methyl isobutyl ketone (MIBK) by gas chromatography and D1364 Test Method for Water in Volatile Solvents (Karl
in addition provides a means for measuring certain impurities Fischer Reagent Titration Method)
such as methyl isobutyl carbinol which are of interest. Impu- D1613 Test Method for Acidity in Volatile Solvents and
rities such as water and acidity are measured by other appro- Chemical Intermediates Used in Paint, Varnish, Lacquer,
priate ASTM procedures and the results are used to normalize and Related Products
the chromatographic value. D2593 Test Method for Butadiene Purity and Hydrocarbon
Impurities by Gas Chromatography
1.2 The following applies to all specified limits in this
E29 Practice for Using Significant Digits in Test Data to
standard; for purposes of determining conformance with this
Determine Conformance with Specifications
standard, an observed value or a calculated value shall be
E180 Practice for Determining the Precision of ASTM
rounded off “to the nearest unit” in the last right-hand digit
Methods for Analysis and Testing of Industrial and Spe-
used in expressing the specification limit, in accordance with
cialty Chemicals (Withdrawn 2009)
the round-off method of Practice E29.
E260 Practice for Packed Column Gas Chromatography
1.3 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information
3. Summary of Test Method
only.
3.1 A representative specimen is introduced onto a gas-
1.4 This standard does not purport to address all of the
liquid partition column. Methyl isobutyl ketone is separated
safety concerns, if any, associated with its use. It is the
from impurities such as acetone, 2-propanol, pentanone, mesi-
responsibility of the user of this standard to establish appro-
tyl oxide, methyl isobutyl carbinol, and several unidentified
priate safety, health, and environmental practices and deter-
compounds as the components are transported through the
mine the applicability of regulatory limitations prior to use.
column by an inert carrier gas. The separated components are
1.5 For specific hazard information and guidance, see the
measured in the effluent by a detector and recorded as a
supplier’s Safety Data Sheet for the materials listed in this test
chromatogram. The chromatogram is interpreted by applying
method.
component attenuation and detector response factors to the
1.6 This international standard was developed in accor-
peak areas, and the relative concentrations are determined by
dance with internationally recognized principles on standard-
relating the individual peak responses to the total peak re-
ization established in the Decision on Principles for the
sponse. Water and acidity are measured in accordance with Test
Development of International Standards, Guides and Recom-
Methods D1364 and D1613 and the results are used to
mendations issued by the World Trade Organization Technical
normalize the values obtained by gas chromatography.
Barriers to Trade (TBT) Committee.
4. Significance and Use
4.1 This test method provides a measurement of commonly
This test method is under the jurisdiction of ASTM Committee D01 on Paint found impurities in commercially available methyl isobutyl
and Related Coatings, Materials, and Applications and is the direct responsibility of
ketone. The measurement of these impurities and the results
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
thereof can individually or when totaled and subtracted from
Current edition approved Dec. 1, 2017. Published December 2017. Originally
100 (assay) be used for specification acceptance.
approved in 1974. Last previous edition approved in 2009 as D3329 – 03 (2009).
DOI: 10.1520/D3329-03R17.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3329 − 03 (2017)
5. Apparatus carrier gas used should be 99.95 mol %. (Warning —If
hydrogen is used, take special safety precautions to ensure that
5.1 Chromatograph—Any gas liquid chromatographic in-
the system is free from leaks and that the effluent is vented
strument having either a thermal conductivity or flame ioniza-
properly.)
tion detector provided the system has sufficient sensitivity and
stability to obtain for 0.01 % of impurity a recorder deflection
6.2 Column Materials:
of at least 2 mm at a signal-to-noise ratio of at least 5 to 1. The
6.2.1 Liquid Phase—The materials successfully used in
specimen size used in judging the sensitivity must be such that
cooperative test work are listed in Table 1. (See Note 1.)
the column is not overloaded, which would result in peak
broadening, loss of resolution, shifting retention times and
NOTE 1—Suppliers of liquid phases and supports can be found in
formation of leading peaks. Research Report RR:D01-1042, available from ASTM International
Headquarters.
5.2 Column—Any column capable of resolving methyl
6.2.2 Solid Support—The materials and their mesh sizes
isobutyl ketone from the impurities that may be present.
successfully used in cooperative work are shown in Table 1.
Possible impurities are hydrocarbons, acetone, 2-propanol,
(See Note 1.)
2-pentanone, 3-pentanone, mesityl oxide, mesityl oxide
isomer, and methyl isobutyl carbinol. Columns that meet this
6.2.3 Tubing Material—Copper, stainless steel, and alumi-
requirement are described in Table 1. Other columns, including
num have been found satisfactory for column tubing. The
capillary columns, may be used, provided the user establishes
tubing must be nonreactive with the substrate, sample, and
that a column gives the required separation and the peak shapes
carrier gas and be of uniform internal diameter.
are satisfactory for measurement so that the precision require-
6.3 Standards for Calibration and Identification—Standard
ments of Section 12 are met.
samples of all components present are needed for identification
5.3 Specimen Introduction System—Any system capable of
by retention time and for calibration for quantitative measure-
introducing a representative specimen onto the column. Mi-
ments.
crolitre syringes have been used successfully.
5.4 Recorder—A recording potentiometer with a full-scale
7. Preparation of Apparatus
deflection of 5 mV or less, full-scale response time of 2 s or
7.1 Column Preparation—The method used to prepare the
less, and sufficient sensitivity and stability to meet the require-
column is not critical provided that the finished column
ments of 5.1.
produces the required separation (Note 2). Partitioning liquids,
6. Reagents and Materials supports, and loading levels used successfully in cooperative
work are listed in Table 1.
6.1 Carrier Gas—Carrier gas appropriate to the type of
detector used. Helium or hydrogen may be employed with
NOTE 2—A suitable method for column preparation is described in Test
thermal conductivity detectors and nitrogen, helium, or argon
Method D2593. Additional useful information may be found in Practice
with flame ionization detectors. The minimum purity of the E260.
TABLE 1 Columns and Conditions Used Successfully in Cooperative Work (See Note 1)
Case I Case II Case III Case IV Case V Case VI
Column:
Liquid phase polyethylene glycol, polyethylene glycol, ethylene oxide/ polyethylene glycol, polyethylene glycol, polyethylene glycol
MW 1450 MW 540 propylene oxide MW 20M
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D3329 − 03 (Reapproved 2009) D3329 − 03 (Reapproved 2017)
Standard Test Method for
1,2
Purity of Methyl Isobutyl Ketone by Gas Chromatography
This standard is issued under the fixed designation D3329; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope*Scope
1.1 This test method covers the determination of the purity of methyl isobutyl ketone (MIBK) by gas chromatography and in
addition provides a means for measuring certain impurities such as methyl isobutyl carbinol which are of interest. Impurities such
as water and acidity are measured by other appropriate ASTM procedures and the results are used to normalize the
chromatographic value.
1.2 The following applies to all specified limits in this standard; for purposes of determining conformance with this standard,
an observed value or a calculated value shall be rounded off “to the nearest unit” in the last right-hand digit used in expressing
the specification limit, in accordance with the round-off method of Practice E29.
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.5 For specific hazard information and guidance, see the supplier’s Material supplier’s Safety Data Sheet for the materials
listed in this test method.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D1364 Test Method for Water in Volatile Solvents (Karl Fischer Reagent Titration Method)
D1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lacquer, and Related
Products
D2593 Test Method for Butadiene Purity and Hydrocarbon Impurities by Gas Chromatography
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals
(Withdrawn 2009)
E260 Practice for Packed Column Gas Chromatography
3. Summary of Test Method
3.1 A representative specimen is introduced onto a gas-liquid partition column. Methyl isobutyl ketone is separated from
impurities such as acetone, 2-propanol, pentanone, mesityl oxide, methyl isobutyl carbinol, and several unidentified compounds
as the components are transported through the column by an inert carrier gas. The separated components are measured in the
effluent by a detector and recorded as a chromatogram. The chromatogram is interpreted by applying component attenuation and
detector response factors to the peak areas, and the relative concentrations are determined by relating the individual peak responses
This test method is under the jurisdiction of ASTM Committee D01 on Paint and Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
Current edition approved Dec. 1, 2009Dec. 1, 2017. Published December 2009December 2017. Originally approved in 1974. Last previous edition approved in 20032009
as D3329 – 03.D3329 – 03 (2009). DOI: 10.1520/D3329-03R09.10.1520/D3329-03R17.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’sstandard’s Document Summary page on the ASTM website.
The last approved version of this historical standard is referenced on www.astm.org.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3329 − 03 (2017)
to the total peak response. Water and acidity are measured in accordance with Test Methods D1364 and D1613 and the results are
used to normalize the values obtained by gas chromatography.
4. Significance and Use
4.1 This test method provides a measurement of commonly found impurities in commercially available methyl isobutyl ketone.
The measurement of these impurities and the results thereof can individually or when totaled and subtracted from 100 (assay) be
used for specification acceptance.
5. Apparatus
5.1 Chromatograph—Any gas liquid chromatographic instrument having either a thermal conductivity or flame ionization
detector provided the system has sufficient sensitivity and stability to obtain for 0.01 % of impurity a recorder deflection of at least
2 mm at a signal-to-noise ratio of at least 5 to 1. The specimen size used in judging the sensitivity must be such that the column
is not overloaded, which would result in peak broadening, loss of resolution, shifting retention times and formation of leading
peaks.
5.2 Column—Any column capable of resolving methyl isobutyl ketone from the impurities that may be present. Possible
impurities are hydrocarbons, acetone, 2-propanol, 2-pentanone, 3-pentanone, mesityl oxide, mesityl oxide isomer, and methyl
isobutyl carbinol. Columns that meet this requirement are described in Table 1. Other columns, including capillary columns, may
be used, provided the user establishes that a column gives the required separation and the peak shapes are satisfactory for
measurement so that the precision requirements of Section 12 are met.
5.3 Specimen Introduction System—Any system capable of introducing a representative specimen onto the column. Microlitre
syringes have been used successfully.
5.4 Recorder—A recording potentiometer with a full-scale deflection of 5 mV or less, full-scale response time of 2 s or less,
and sufficient sensitivity and stability to meet the requirements of 5.1.
6. Reagents and Materials
6.1 Carrier Gas—Carrier gas appropriate to the type of detector used. Helium or hydrogen may be employed with thermal
conductivity detectors and nitrogen, helium, or argon with flame ionization detectors. The minimum purity of the carrier gas used
should be 99.95 mol %. (Warning —If hydrogen is used, take special safety precautions to ensure that the system is free from
leaks and that the effluent is vented properly.)
6.2 Column Materials:
6.2.1 Liquid Phase—The materials successfully used in cooperative test work are listed in Table 1. (See Note 1.)
TABLE 1 Columns and Conditions Used Successfully in Cooperative Work (See Note 1)
Case I Case II Case III Case IV Case V Case VI
Column:
Liquid phase polyethylene glycol, polyethylene glycol, ethylene oxide/ polyethylene glycol, polyethylene glycol, polyethylene glycol
MW 1450 MW 540 propylene oxide MW 20M MW 3350
copolymer
Liquid phase, weight % 15 20 20 25 25 1.2 μm film
Support diatomaceous earth, diatomaceous earth diatomaceous earth, diatomaceous earth diatomaceous earth capillary
acid washed acid washed
Support mesh size 60 to 80 60 to 80 45 to 60 60 to 80 60 to 80 N/A
Length, m (ft) 6.1 (20) 5.5 (18) 6.1 (20) 3.0 (10) 3.7 (12) 10 (33)
1 1 1 1 1
Diameter, mm (in.) 3.2 ( ⁄8 ) 6.4 ( ⁄4 ) 6.4 ( ⁄4 ) 3.2 ( ⁄8 ) 6.4 ( ⁄4 ) 0.53 (0.021)
Temperature, °C 90 100 160 75 to 200 145 40 to 180 at
programmed at 5°/min
4°/min
Carrier gas: helium helium helium helium helium helium
Flow rate, mL/min 30 50 60 20 80 5
Typical retention time, min:
Methyl isobutyl ketone 9.3 27.2 8.1 11.2 7.7 1.84
Relative retention time,
MIBK = 1.00:
Acetone 0.42 0.39 0.52 0.42 0.39 0.36
2-propanol 0.66 0.57 0.65 0.56 0.59
2- and 3-pentanone 0.85 0.82 0.78 . . 0.79
Methyl isobutyl ketone 1.00 1.00 1.00 1.00 1.00 1.00
α-Mesityl oxide 1.45 1.41 1.27 . . .
β-Mesityl oxide 1.89 1.85 1.63 1.24 1.52 .
Methyl isobutyl carbinol 2.11 2.07 1.48 1.42 1.95 2.24
D3329 − 03 (2017)
NOTE 1—Supplie
...
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